Robust Optimization of Chaotropic Chromatography Assay for Lamotrigine and its Two Impurities in Tablets

Development of Analytical Quality by Design Compliant Chaotropic Chromatography Method for Ziprasidone and Its Five Impurities Determination

“…The objective of this research was to efficiently develop a reliable and robust method for the analysis of ZPS and its five impurities using the AQbD approach, also known as robust optimization [ 18 ]. In developing analytical methods using the AQbD principles, the analytical target profile (ATP) must first be defined.…”

“…ZPS and its five impurities are substances with basic character. Based on our previous experience with such solutes [ 18 , 20 , 21 ], we decided to add column friendly chaotropic reagents to the mobile phase to achieve appropriate peak shape and retention. Anions, which are commonly part of the mobile phase in chaotropic chromatography, are hexafluorophosphate, perchlorate, or trifluoroacetate.…”

“…The plan of experiments and experimentally obtained responses are shown in Table 4 . The resulting main effects models had acceptable statistical parameters, and the estimates for dummy factor effects were not statistically significant, indicating that no inestimable interactions were leaking into the estimable effects [ 18 ]. Only two quantitative responses, P _imp II and P _imp V , were found to be significantly affected, the first by mobile phase flow rate ( N ) and the second by gradient duration ( D ).…”

Chaotropic chromatography method development for the determination of aripiprazole and its impurities following analytical quality by design principles

“…For the detection of important interactions in so called main effect experimental plans like Plackett–Burman design, we applied approach thoroughly described in Čolović et al. [21]. First of all, alias matrix was constructed, then the potential contribution of any inestimable interactions to all the large effects was evaluated and Lawson alias plot created for visualization of the potential contribution of each inestimable interaction to the largest estimated effects (Figure S2).…”

“…Among all the points included in DS, working point was selected and robustness of quantitative performances of developed method was studied employing the approach described in Čolović et al. [21]. Finally, developed method was validated to demonstrate its suitability for intended purpose.…”